CN110692627A - Attapulgite clay powder for pesticide carrier and preparation method thereof - Google Patents
Attapulgite clay powder for pesticide carrier and preparation method thereof Download PDFInfo
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- CN110692627A CN110692627A CN201910846192.0A CN201910846192A CN110692627A CN 110692627 A CN110692627 A CN 110692627A CN 201910846192 A CN201910846192 A CN 201910846192A CN 110692627 A CN110692627 A CN 110692627A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/44—Products obtained from layered base-exchange silicates by ion-exchange with organic compounds such as ammonium, phosphonium or sulfonium compounds or by intercalation of organic compounds, e.g. organoclay material
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Abstract
The invention belongs to the technical field of clay powder preparation, and discloses attapulgite clay powder for a pesticide carrier and a preparation method thereof, wherein the attapulgite clay powder for the pesticide carrier comprises the following components: 20 parts of purified attapulgite clay, 25 parts of montmorillonite, 15 parts of fly ash, 6 parts of calcium silicate, 2 parts of hydroxypropyl methyl cellulose, 5 parts of sodium dodecyl sulfate, 22 parts of bentonite, 2 parts of aluminum oxide, 3 parts of sodium dodecyl benzene sulfonate, 4 parts of sodium tripolyphosphate, 6 parts of soybean straw powder, 10 parts of adhesive, 4 parts of emulsifier, 6 parts of defoaming agent, 10 parts of corn starch, 7 parts of wetting agent and water. The purity of the attapulgite clay obtained by the purification method of the attapulgite clay provided by the invention is up to more than 99.5%; meanwhile, the attapulgite clay powder modification method can inhibit the polymerization reaction among the attapulgite clay powder and improve the compatibility and the dispersibility of the attapulgite clay powder in the alcohol-based solution.
Description
Technical Field
The invention belongs to the technical field of clay powder preparation, and particularly relates to attapulgite clay powder for a pesticide carrier and a preparation method thereof.
Background
Attapulgite, also known as Palygorskite (Palygorskite) or Palygorskite, is an aqueous magnesium-rich aluminosilicate clay mineral with a chain-layered structure. The structure of the mineral belongs to 2:1 type clay minerals. In each 2:1 unit structure layer, the tetrahedral wafer angular tips are reversed at a certain distance to form a chain. Channels parallel to the chain are formed between the tetrahedral strips, the cross-section of the channels being about
The channels are filled with zeolite water and crystal water, which are shown in the structure diagram of attapulgite clay crystals. The attapulgite clay is a clay mineral containing attapulgite (Attapulgite) as main component. Attapulgite is a crystalline hydrated magnesium aluminum silicate mineral, has unique layer chain structure characteristics, has lattice displacement in the structure, and contains variable amount of Na in the crystal+、Ca2+、Fe3+、Al3+The crystals are needle-shaped, fibrous or fibrous aggregates. The attapulgite has good colloidal properties of unique dispersion, high temperature resistance, salt and alkali resistance and the like and higher adsorption decoloring capacity. The adhesive has certain plasticity and binding power, and the ideal chemical molecular formula is as follows: MgAl5Si8O20(OH)2(OH2)4·4H2And O. Having an intermediate structure between the chain-like structure and the layered structure. The attapulgite is in the form of soil and compact blockThe color of the product is white, grey, grey green or weak silk luster. The soil is fine and smooth, has a greasy feeling, is light and crisp, has shell-shaped or ragged fracture and strong water absorption. Has viscosity and plasticity when wet, shrinks less after drying, does not show cracks greatly, and is soaked in water to be disintegrated. The suspension does not flocculate and precipitate when encountering dielectrics. However,
in summary, the problems of the prior art are as follows:
the existing attapulgite clay is difficult to fully suspend in aqueous solution, and the surface is easy to generate polymerization reaction to form dead condensation, thereby influencing the purification effect; meanwhile, the surface of the attapulgite clay contains a large number of hydroxyl groups and negative charges, so that the attapulgite clay is hydrophilic, is difficult to disperse in an organic system and cannot embody the special functions of the attapulgite clay. In order to improve the compatibility and dispersibility of the attapulgite in organic systems, the attapulgite must be subjected to organic surface modification. The existing hydroxypropyl methyl cellulose has poor dissolving performance and incomplete reaction; the existing sodium tripolyphosphate is not high in solubility, and the reaction rate and the product solubility are influenced in actual production.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides attapulgite clay powder for a pesticide carrier and a preparation method thereof.
The invention is realized in such a way that the attapulgite clay powder for the pesticide carrier consists of the following components:
20 parts of purified attapulgite clay, 25 parts of montmorillonite, 15 parts of fly ash, 6 parts of calcium silicate, 2 parts of hydroxypropyl methyl cellulose, 5 parts of sodium dodecyl sulfate, 22 parts of bentonite, 2 parts of aluminum oxide, 3 parts of sodium dodecyl benzene sulfonate, 4 parts of sodium tripolyphosphate, 6 parts of soybean straw powder, 10 parts of adhesive, 4 parts of emulsifier, 6 parts of defoaming agent, 10 parts of corn starch, 7 parts of wetting agent and water.
Furthermore, the addition amount of the water is selected according to the actual production requirement.
Further, the adhesive consists of 3 parts of octyl acrylate, 2 parts of butyl acrylate, 3 parts of acrylic acid, 2 parts of hydroxyethyl acrylate, 1 part of ethyl acetate and 8 parts of deionized water in parts by mass; weighing the raw materials in the proportion, and then putting paraffin into a reaction kettle, adding deionized water, heating and emulsifying; then adding octyl acrylate, butyl acrylate, acrylic acid, hydroxyethyl acrylate and ethyl acetate according to the proportion, and then uniformly stirring; and finally, heating the reaction kettle to 60-100 ℃, and stirring to obtain the adhesive.
Further, the emulsifier comprises the following components in percentage by mass:
23-45% of water, 8-12% of glycol, 22-32% of fatty alcohol-polyoxyethylene ether and 8-15% of polyethylene glycol distearate.
Further, the defoaming agent consists of, by mass: 5g of methyl silane oil, 5g of sodium tripolyphosphate, 20g of salt, 1g of mannitol and 2g of silicon dioxide; mixing methyl siloxane oil and silicon dioxide at room temperature; and mixing the crushed sodium tripolyphosphate, the mannitol and the salt, adding the mixture into the mixture of the methyl siloxane oil and the silicon dioxide, and fully stirring the mixture to obtain the defoaming agent.
Further, the wetting agent is one of anionic surfactant, nonionic surfactant and silanol nonionic surfactant.
The anionic surfactant comprises one of alkyl sulfate, sulfonate, fatty acid or fatty acid ester sulfate, carboxylic acid soap and phosphate.
The nonionic surfactant comprises one of polyoxyethylene alkylphenol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene polyoxypropylene block copolymer.
The invention also aims to provide a preparation method of the attapulgite clay powder for the pesticide carrier, which comprises the following steps:
crushing purified attapulgite clay, montmorillonite, fly ash and calcium silicate, adding hydroxypropyl methyl cellulose, sodium dodecyl sulfate, bentonite, aluminum oxide, sodium dodecyl benzene sulfonate, sodium tripolyphosphate, soybean straw powder, an adhesive, an emulsifier, a defoaming agent, corn starch, a wetting agent and water, mixing and stirring, and performing ultrasonic treatment for 25 minutes;
step two, adding the mixture into a kiln and drying until the moisture content is less than 5%;
step three, uniformly, quantitatively and continuously feeding the dry mixture into a grinding chamber of a main machine of a pulverizer to grind, wherein the grinding time is between 0.3, and the grinding temperature is between 56 ℃, so that attapulgite clay powder is obtained;
and step four, modifying the obtained attapulgite clay powder, grading by using a powder concentrator, and packaging the collected modified attapulgite clay powder by using a packaging machine to obtain a finished product.
Further, the method for purifying attapulgite clay in the first step comprises the following steps:
A. weighing 50g of attapulgite clay, placing the attapulgite clay into 900mL of distilled water, stirring the attapulgite clay for 3 hours at 1500 rpm by using a cross stirring blade stirrer, and activating the attapulgite clay in 50mL of hydrochloric acid with the concentration of lmol/L in a water bath at 85 ℃ for 2 hours; adding 6mL of active agent into the activated suspension, adding NaOH solution to adjust the pH value of the suspension to 7, stirring for 3 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, separating the attapulgite clay suspension and a deposited impurity layer, and filtering out impurities;
B. adding 4g of organic salt into the separated attapulgite clay suspension, reacting for 10 minutes, centrifuging the reaction solution in a centrifuge for 4 times, each time for 5 minutes, and recovering solid;
C. adding 14g of inorganic salt into the recovered solid, adding distilled water to 1000mL to prepare a suspension, heating the prepared suspension to 80 ℃, preserving heat for 5 hours, then carrying out centrifugal treatment on the heat-preserved suspension at a rotating speed of 3500r/min for 3 times, carrying out centrifugal separation for 5 minutes each time, further recovering the solid, and drying at 70-100 ℃ for 24 hours to obtain purified attapulgite clay;
wherein, the active agent in the step A is selected from alkylphenol polyoxyethylene ether type active agent, sorbitan fatty acid ester type active agent or tween-20 type active agent; b, selecting ethylene diamine tetraacetic acid disodium salt as the organic salt; the inorganic salt in the step C is Na2CO3。
Further, the method for modifying the attapulgite clay powder in the fourth step comprises the following steps:
(1) adding nano SiO into attapulgite clay powder2Adding water, stirring for 3 hours in a water bath at 60 ℃, standing for 2 hours, and drying to obtain powder; the fineness of the attapulgite clay powder is 300 meshes; the nano-scale SiO2The weight of the particles accounts for 15 percent of the weight of the attapulgite clay powder; the addition amount of the water is based on the weight of the attapulgite clay powder, and 4ml of water is added into each gram of the attapulgite clay powder;
(2) adding the composite modifier into the powder prepared in the step (1), stirring at a high speed of 188r/min by using a planetary mill for 5 hours, and then sealing and standing for 6 hours to prepare slurry; the addition amount of the composite modifier is 4 percent of the weight of the attapulgite clay powder; the composite modifier is stearic acid and a polyoxyethylene oleyl ether surfactant, and the volume ratio of the stearic acid to the polyoxyethylene oleyl ether surfactant is 1: 1-1: 2;
(3) and (3) filtering the slurry prepared in the step (2), washing the powder for multiple times by adopting an organic solvent absolute ethyl alcohol, and drying by using a vacuum drying oven at the temperature of 90 ℃ for 4 hours to obtain the modified attapulgite clay powder.
The invention has the advantages and positive effects that:
according to the method for purifying the attapulgite clay, the active agent is adsorbed on the surface of the attapulgite clay, so that the attapulgite clay powder is fully dispersed in water, and the disodium ethylene diamine tetraacetate can form a complex with calcium and magnesium ions to promote the dissolution of carbonate so as to remove the carbonate without changing the property and the structure of the attapulgite; adding Na into attapulgite clay powder2CO3And heating to 70-100 ℃ and Na2CO3Exchanging Na ions with Ca ions in the evenly dispersed attapulgite clay suspension to generate CaCO3Precipitating, and removing Ca ions in the attapulgite clay suspension; removing high-density quartz by centrifugation, filtering the final suspension, drying to obtain high-purity attapulgite clay powder, analyzing the powder purity by XRD and TEM energy spectrum, and measuring and calculating the percentage content of its main compounds to obtain the final productThe purity of the attapulgite clay is as high as more than 99.5 percent; meanwhile, the attapulgite clay powder modification method utilizes the high activity of the nano inorganic particles to make the nano inorganic particles adsorbed on the surface of the attapulgite clay powder, thereby preventing the reaction between the attapulgite clay powder; then, a layer of composite activator mixed by organic carboxylic acid and nonionic surfactant is coated on the surface of the attapulgite powder, which can inhibit the polymerization reaction between the attapulgite powder and improve the compatibility and the dispersibility of the attapulgite powder in alcohol-based solution.
The hydroxypropyl methyl cellulose prepared by the preparation method provided by the invention has high solubility and can be reacted uniformly. The sodium tripolyphosphate prepared by the preparation method provided by the invention has no influence on the solubility of the attapulgite clay powder used as a pesticide carrier, and the production process is simple and controllable and has good solubility.
The emulsifier has strong emulsifying capacity, saves production time and is environment-friendly.
The adhesive disclosed by the invention is simple in preparation method, non-toxic, environment-friendly, high in safety and suitable for long-term storage. The invention has wide source and low cost, and is suitable for large-scale production.
Drawings
Fig. 1 is a flow chart of a method for preparing attapulgite clay powder for a pesticide carrier according to an embodiment of the invention.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are exemplified and included in the detailed description with reference to the accompanying drawings.
The existing attapulgite clay is difficult to fully suspend in aqueous solution, and the surface is easy to generate polymerization reaction to form dead condensation, thereby influencing the purification effect; meanwhile, the surface of the attapulgite clay contains a large number of hydroxyl groups and negative charges, so that the attapulgite clay is hydrophilic, is difficult to disperse in an organic system and cannot embody the special functions of the attapulgite clay. In order to improve the compatibility and dispersibility of the attapulgite in organic systems, the attapulgite must be subjected to organic surface modification. The existing hydroxypropyl methyl cellulose has poor dissolving performance and incomplete reaction; the existing sodium tripolyphosphate is not high in solubility, and the reaction rate and the product solubility are influenced in actual production.
To solve the above problems, the present invention will be described in detail with reference to the accompanying drawings.
The attapulgite clay powder for the pesticide carrier provided by the embodiment of the invention comprises, by mass, 20-30 parts of purified attapulgite clay, 15-20 parts of montmorillonite, 10-15 parts of fly ash, 6-8 parts of calcium silicate, 2-4 parts of hydroxypropyl methyl cellulose, 5-8 parts of sodium dodecyl sulfate, 6-8 parts of bentonite, 2-4 parts of aluminum oxide, 3-5 parts of sodium dodecyl benzene sulfonate, 4-6 parts of sodium tripolyphosphate, 6-8 parts of soybean straw powder, 6-9 parts of an adhesive, 2-4 parts of an emulsifier, 5-8 parts of a defoaming agent, 5-7 parts of corn starch, 3-5 parts of a wetting agent and water.
The addition amount of the water is selected according to the actual production requirement.
The adhesive consists of 3 parts of octyl acrylate, 2 parts of butyl acrylate, 3 parts of acrylic acid, 2 parts of hydroxyethyl acrylate, 1 part of ethyl acetate and 8 parts of deionized water in parts by mass; weighing the raw materials in the proportion, and then putting paraffin into a reaction kettle, adding deionized water, heating and emulsifying; then adding octyl acrylate, butyl acrylate, acrylic acid, hydroxyethyl acrylate and ethyl acetate according to the proportion, and then uniformly stirring; and finally, heating the reaction kettle to 60-100 ℃, and stirring to obtain the adhesive.
The emulsifier comprises the following components in percentage by mass:
23-45% of water, 8-12% of glycol, 22-32% of fatty alcohol-polyoxyethylene ether and 8-15% of polyethylene glycol distearate.
The defoaming agent comprises the following components in percentage by mass: 5g of methyl silane oil, 5g of sodium tripolyphosphate, 20g of salt, 1g of mannitol and 2g of silicon dioxide; mixing methyl siloxane oil and silicon dioxide at room temperature; and mixing the crushed sodium tripolyphosphate, the mannitol and the salt, adding the mixture into the mixture of the methyl siloxane oil and the silicon dioxide, and fully stirring the mixture to obtain the defoaming agent.
The wetting agent is one of anionic surfactant, nonionic surfactant and silanol nonionic surfactant.
The anionic surfactant comprises one of alkyl sulfate, sulfonate, fatty acid or fatty acid ester sulfate, carboxylic acid soap and phosphate.
The nonionic surfactant comprises one of polyoxyethylene alkylphenol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene polyoxypropylene block copolymer.
The silanol nonionic surfactant, also called wetting agent, is characterized by low molecular weight, umbrella-shaped symmetrical multi-hydrophobic group structure, excellent wetting and permeability performance and high efficiency compared with the traditional surfactant, and is a revolutionary new-generation surfactant. The active and static surface tension is extremely low, the active agent contains dihydroxyl group, the reactive active agent is inert in chemical property, does not participate in the chemical reaction of the system generally, and has good acid and alkali resistance and stable chemical property. The model is typically GSK-588/582/585 series.
The wetting agent is composed of hydrophilic group and lipophilic group, when the wetting agent is contacted with solid surface, the hydrophilic group is attached to the solid surface, and the lipophilic group is extended outwards to the liquid, so that the liquid forms continuous phase on the solid surface, which is the basic principle of wetting action
In general, the wetting agent is usually used for wetting drugs with low hydrophobicity by grinding with ethanol, propylene glycol, glycerol, etc.; for drugs or medicinal materials with strong hydrophobicity, a surfactant with the HLB value of 6-15 is generally selected. The selection can also be made by any of the following criteria:
contact angles (contact angles) are the angle between the droplet and the spreading surface, and the wetting agent is chosen to reduce the contact angle of the hydrophobic drug to less than 90 °. When the contact angle is 0, the paint can be completely wetted; the contact angle is 0-90 degrees, the wetting can be realized, and the drug is hydrophilic; the contact angle is more than 90 degrees and less than 180 degrees, and the paint cannot be wetted; the contact angle is 180 degrees, the medicine is completely non-wetting and is hydrophobic.
Interfacial tensions certain wetting agents alter the interfacial tension of hydrophobic drugs and solvents.
Wetting Point-wetting Point is the amount of solvent required to just wet 100g of hydrophobic drug, and the addition of a wetting agent allows the wetting point to be lowered, i.e., the amount of solvent used to be reduced.
As shown in fig. 1, the preparation method of the attapulgite clay powder for pesticide carriers provided by the embodiment of the invention comprises the following steps:
s101, carrying out ultrasonic crushing on the purified attapulgite clay, montmorillonite, fly ash and calcium silicate, then adding hydroxypropyl methyl cellulose, sodium dodecyl sulfate, bentonite, aluminum oxide, sodium dodecyl benzene sulfonate, sodium tripolyphosphate, soybean straw powder, an adhesive, an emulsifier, a defoaming agent, corn starch, a wetting agent and water, mixing and stirring, and carrying out ultrasonic treatment for 25 minutes.
And S102, adding the mixture into a kiln, and drying until the moisture is less than 5%.
S103, uniformly, quantitatively and continuously feeding the dry mixture into a main grinding chamber of a pulverizer to grind, wherein the grinding time is between 0.3, and the grinding temperature is between 56 ℃, so that the attapulgite clay powder is obtained.
S104, modifying the obtained attapulgite clay powder, grading by using a powder concentrator, and packaging the collected modified attapulgite clay powder by using a packaging machine to obtain a finished product.
In step S101, the method for purifying attapulgite clay according to the embodiment of the present invention includes:
A. weighing 50g of attapulgite clay, placing the attapulgite clay into 900mL of distilled water, stirring the attapulgite clay for 3 hours at 1500 rpm by using a cross stirring blade stirrer, and activating the attapulgite clay in 50mL of hydrochloric acid with the concentration of lmol/L in a water bath at 85 ℃ for 2 hours; adding 6mL of active agent into the activated suspension, adding NaOH solution to adjust the pH value of the suspension to 7, stirring for 3 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, separating the attapulgite clay suspension and the deposited impurity layer, and filtering out impurities.
B. Adding 4g of organic salt into the separated attapulgite clay suspension, reacting for 10 min, centrifuging the reaction solution in a centrifuge for 5 min for 4 times, and recovering solid.
C. Adding 14g of inorganic salt into the recovered solid, adding distilled water to 1000mL to prepare a suspension, heating the prepared suspension to 80 ℃, preserving heat for 5 hours, then carrying out centrifugal treatment on the heat preserved suspension at the rotating speed of 3500r/min for 3 times, carrying out centrifugal separation for 5 minutes each time, further recovering the solid, and drying at 70-100 ℃ for 24 hours to obtain the purified attapulgite clay.
In step a, the active agent provided in the embodiment of the present invention is an alkylphenol polyoxyethylene ether type active agent, a sorbitan fatty acid ester type active agent, or a tween-20 type active agent.
In the step B, the organic salt provided by the embodiment of the present invention is ethylenediaminetetraacetic acid disodium salt.
In step C, Na is selected as the inorganic salt provided by the embodiment of the invention2CO3。
In step S101, the method for preparing hydroxypropylmethylcellulose provided by the embodiment of the present invention includes:
(1) adding cellulose pulp into a solvent containing a phase transfer catalyst, adding sodium hydroxide, propylene oxide and methyl chloride for permeation, and performing etherification reaction to obtain a hydroxypropyl methyl cellulose crude product.
(2) And recovering the solvent used in the etherification reaction process through desolventizing.
(3) Separating the hydroxypropyl methyl cellulose crude product and water by filtering and washing and removing impurities in the hydroxypropyl methyl cellulose crude product.
(4) Spraying glyoxal water solution on the filtered and washed material for crosslinking treatment;
(5) the material after the cross-linking treatment enters a granulator for extrusion granulation, and the granulated material is cooled;
(6) and pre-crushing, drying and crushing the granulated material to obtain a hydroxypropyl methyl cellulose product.
In step S101, the method for preparing sodium tripolyphosphate provided by the embodiment of the present invention includes:
1) the ingredients of potassium tripolyphosphate, sodium pyrophosphate and sodium hexametaphosphate were mixed and then premixed for 30 minutes using a high speed mixer.
2) And (3) mixing the sodium tripolyphosphate into the premix by using a high-speed mixer, and fully mixing for 10-20 minutes at the mixing temperature of below 40 ℃.
3) And (3) passing the material obtained in the step (2) through a 18-mesh screen to obtain the sodium tripolyphosphate.
In step S104, the method for modifying attapulgite clay powder according to the embodiment of the present invention includes:
(1) adding nano SiO into attapulgite clay powder2Adding water, stirring in water bath at 60 deg.C for 3 hr, standing for 2 hr, and oven drying to obtain powder. The fineness of the attapulgite clay powder is 300 meshes. The nano-scale SiO2The weight of the particles is 15% of the weight of the attapulgite clay powder. The addition amount of the water is based on the weight of the attapulgite clay powder, and 4ml of water is added into each gram of the attapulgite clay powder.
(2) Adding the composite modifier into the powder prepared in the step (1), stirring at a high speed of 188r/min by using a planetary mill for 5 hours, and then sealing and standing for 6 hours to prepare slurry. The addition amount of the composite modifier is 4 percent of the weight of the attapulgite clay powder. The composite modifier is stearic acid and a polyoxyethylene oleyl ether surfactant, and the volume ratio of the stearic acid to the polyoxyethylene oleyl ether surfactant is 1: 1-1: 2.
(3) And (3) filtering the slurry prepared in the step (2), washing the powder for multiple times by adopting an organic solvent absolute ethyl alcohol, and drying by using a vacuum drying oven at the temperature of 90 ℃ for 4 hours to obtain the modified attapulgite clay powder.
The technical solution and technical effects of the present invention are further described below with reference to specific embodiments.
Example 1:
step one, crushing 20 parts of purified attapulgite clay, 15 parts of montmorillonite, 10 parts of fly ash and 6 parts of calcium silicate, adding 2 parts of hydroxypropyl methyl cellulose, 5 parts of sodium dodecyl sulfate, 6 parts of bentonite, 2 parts of alumina, 3 parts of sodium dodecyl benzene sulfonate, 4 parts of sodium tripolyphosphate, 6 parts of soybean straw powder, 6 parts of an adhesive, 2 parts of an emulsifier, 5 parts of a defoaming agent, 5 parts of corn starch, 3 parts of a wetting agent and water, mixing and stirring, and performing ultrasonic treatment for 25 minutes.
And step two, adding the mixture into a kiln and drying until the moisture content is less than 5%.
And step three, uniformly, quantitatively and continuously feeding the dry mixture into a grinding chamber of a main machine of the pulverizer to grind, wherein the grinding time is between 0.3, and the grinding temperature is between 56 ℃, so as to obtain the attapulgite clay powder.
And step four, modifying the obtained attapulgite clay powder, grading by using a powder concentrator, and packaging the collected modified attapulgite clay powder by using a packaging machine to obtain a finished product.
Example 2:
step one, crushing 25 parts of purified attapulgite clay, 17 parts of montmorillonite, 13 parts of fly ash and 7 parts of calcium silicate, adding 3 parts of hydroxypropyl methyl cellulose, 6 parts of sodium dodecyl sulfate, 7 parts of bentonite, 3 parts of alumina, 4 parts of sodium dodecyl benzene sulfonate, 5 parts of sodium tripolyphosphate, 7 parts of soybean straw powder, 7 parts of adhesive, 3 parts of emulsifier, 7 parts of defoamer, 6 parts of corn starch, 4 parts of wetting agent and water, mixing and stirring, and performing ultrasonic treatment for 25 minutes.
And step two, adding the mixture into a kiln and drying until the moisture content is less than 5%.
And step three, uniformly, quantitatively and continuously feeding the dry mixture into a grinding chamber of a main machine of the pulverizer to grind, wherein the grinding time is between 0.3, and the grinding temperature is between 56 ℃, so as to obtain the attapulgite clay powder.
And step four, modifying the obtained attapulgite clay powder, grading by using a powder concentrator, and packaging the collected modified attapulgite clay powder by using a packaging machine to obtain a finished product.
Example 3:
step one, crushing 30 parts of purified attapulgite clay, 20 parts of montmorillonite, 15 parts of fly ash and 8 parts of calcium silicate, adding 4 parts of hydroxypropyl methyl cellulose, 8 parts of sodium dodecyl sulfate, 8 parts of bentonite, 4 parts of alumina, 5 parts of sodium dodecyl benzene sulfonate, 6 parts of sodium tripolyphosphate, 8 parts of soybean straw powder, 9 parts of an adhesive, 4 parts of an emulsifier, 8 parts of a defoaming agent, 7 parts of corn starch, 5 parts of a wetting agent and water, mixing and stirring, and performing ultrasonic treatment for 25 minutes.
And step two, adding the mixture into a kiln and drying until the moisture content is less than 5%.
And step three, uniformly, quantitatively and continuously feeding the dry mixture into a grinding chamber of a main machine of the pulverizer to grind, wherein the grinding time is between 0.3, and the grinding temperature is between 56 ℃, so as to obtain the attapulgite clay powder.
And step four, modifying the obtained attapulgite clay powder, grading by using a powder concentrator, and packaging the collected modified attapulgite clay powder by using a packaging machine to obtain a finished product.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (10)
1. The attapulgite clay powder for the pesticide carrier is characterized by comprising the following components in parts by mass:
20 parts of purified attapulgite clay, 25 parts of montmorillonite, 15 parts of fly ash, 6 parts of calcium silicate, 2 parts of hydroxypropyl methyl cellulose, 5 parts of sodium dodecyl sulfate, 22 parts of bentonite, 2 parts of aluminum oxide, 3 parts of sodium dodecyl benzene sulfonate, 4 parts of sodium tripolyphosphate, 6 parts of soybean straw powder, 10 parts of adhesive, 4 parts of emulsifier, 6 parts of defoaming agent, 10 parts of corn starch, 7 parts of wetting agent and water.
2. The attapulgite clay powder for pesticide carriers according to claim 1, wherein the addition amount of the water is selected according to actual production requirements.
3. The attapulgite clay powder for pesticide carriers according to claim 1, wherein the binder consists of 3 parts by mass of octyl acrylate, 2 parts by mass of butyl acrylate, 3 parts by mass of acrylic acid, 2 parts by mass of hydroxyethyl acrylate, 1 part by mass of ethyl acetate and 8 parts by mass of deionized water; weighing the raw materials in the proportion, and then putting paraffin into a reaction kettle, adding deionized water, heating and emulsifying; then adding octyl acrylate, butyl acrylate, acrylic acid, hydroxyethyl acrylate and ethyl acetate according to the proportion, and then uniformly stirring; and finally, heating the reaction kettle to 60-100 ℃, and stirring to obtain the adhesive.
4. The attapulgite clay powder for pesticide carriers according to claim 1, wherein the emulsifier consists of the following components by mass:
23-45% of water, 8-12% of glycol, 22-32% of fatty alcohol-polyoxyethylene ether and 8-15% of polyethylene glycol distearate.
5. The attapulgite clay powder for pesticide carriers according to claim 1, wherein the antifoaming agent consists of, by mass: 5g of methyl silane oil, 5g of sodium tripolyphosphate, 20g of salt, 1g of mannitol and 2g of silicon dioxide; mixing methyl siloxane oil and silicon dioxide at room temperature; and mixing the crushed sodium tripolyphosphate, the mannitol and the salt, adding the mixture into the mixture of the methyl siloxane oil and the silicon dioxide, and fully stirring the mixture to obtain the defoaming agent.
6. The attapulgite clay powder for pesticide carriers according to claim 1, wherein the wetting agent is one of anionic, nonionic and silanol nonionic surfactants;
the anionic surfactant comprises one of alkyl sulfate, sulfonate, fatty acid or fatty acid ester sulfate, carboxylic acid soap and phosphate;
the nonionic surfactant comprises one of polyoxyethylene alkylphenol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene polyoxypropylene block copolymer.
7. The method for preparing the attapulgite clay powder for pesticide carriers according to claim 1, which is characterized by comprising the following steps:
crushing purified attapulgite clay, montmorillonite, fly ash and calcium silicate, adding hydroxypropyl methyl cellulose, sodium dodecyl sulfate, bentonite, aluminum oxide, sodium dodecyl benzene sulfonate, sodium tripolyphosphate, soybean straw powder, an adhesive, an emulsifier, a defoaming agent, corn starch, a wetting agent and water, mixing and stirring, and performing ultrasonic treatment for 25 minutes;
step two, adding the mixture into a kiln and drying until the moisture content is less than 5%;
step three, uniformly, quantitatively and continuously feeding the dry mixture into a main grinding chamber of a pulverizer to grind for 0.3 hour at the grinding temperature of 56 ℃ to obtain attapulgite clay powder;
and step four, modifying the obtained attapulgite clay powder, grading by using a powder concentrator, and packaging the collected modified attapulgite clay powder by using a packaging machine to obtain a finished product.
8. The method for preparing attapulgite clay powder for pesticide carriers according to claim 7, wherein the method for purifying attapulgite clay in the first step comprises:
A. weighing 50g of attapulgite clay, placing the attapulgite clay into 900mL of distilled water, stirring the attapulgite clay for 3 hours at 1500 rpm by using a cross stirring blade stirrer, and activating the attapulgite clay in 50mL of hydrochloric acid with the concentration of lmol/L in a water bath at 85 ℃ for 2 hours; adding 6mL of active agent into the activated suspension, adding NaOH solution to adjust the pH value of the suspension to 7, stirring for 3 hours at 1500 rpm by using a cross stirring blade stirrer, standing for 10 hours, separating the attapulgite clay suspension and a deposited impurity layer, and filtering out impurities;
B. adding 4g of organic salt into the separated attapulgite clay suspension, reacting for 10 minutes, centrifuging the reaction solution in a centrifuge for 4 times, each time for 5 minutes, and recovering solid;
C. adding 14g of inorganic salt into the recovered solid, adding distilled water to 1000mL to prepare a suspension, heating the prepared suspension to 80 ℃, preserving heat for 5 hours, then carrying out centrifugal treatment on the heat preserved suspension at the rotating speed of 3500r/min for 3 times, carrying out centrifugal separation for 5 minutes each time, further recovering the solid, and drying at 70-100 ℃ for 24 hours to obtain the purified attapulgite clay.
9. The method for preparing attapulgite clay powder for pesticide carriers according to claim 8, wherein the active agent in the step A is selected from alkylphenol polyoxyethylene ether type active agent, sorbitan fatty acid ester type active agent or tween-20 type active agent; b, selecting ethylene diamine tetraacetic acid disodium salt as the organic salt; the inorganic salt in the step C is Na2CO3。
10. The method for preparing attapulgite clay powder for pesticide carriers according to claim 3, wherein the method for modifying the attapulgite clay powder in the fourth step comprises the following steps:
(1) adding nano SiO into attapulgite clay powder2Adding water, stirring for 3 hours in a water bath at 60 ℃, standing for 2 hours, and drying to obtain powder; the fineness of the attapulgite clay powder is 300 meshes; the nano-scale SiO2The weight of the particles accounts for 15 percent of the weight of the attapulgite clay powder; the addition amount of the water is based on the weight of the attapulgite clay powder, and 4ml of water is added into each gram of the attapulgite clay powder;
(2) adding the composite modifier into the powder prepared in the step (1), stirring at a high speed of 188r/min by using a planetary mill for 5 hours, and then sealing and standing for 6 hours to prepare slurry; the addition amount of the composite modifier is 4 percent of the weight of the attapulgite clay powder;
the composite modifier is stearic acid and a polyoxyethylene oleyl ether surfactant, and the volume ratio of the stearic acid to the polyoxyethylene oleyl ether surfactant is 1: 1-1: 2;
(3) and (3) filtering the slurry prepared in the step (2), washing the powder for multiple times by adopting an organic solvent absolute ethyl alcohol, and drying by using a vacuum drying oven at the temperature of 90 ℃ for 4 hours to obtain the modified attapulgite clay powder.
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